CN114047213A - Method for measuring weight of zinc layer by X-ray fluorescence method - Google Patents
Method for measuring weight of zinc layer by X-ray fluorescence method Download PDFInfo
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Abstract
The invention discloses a method for measuring the weight of a zinc layer by an X-ray fluorescence method, which relates to the technical field of metallurgical material analysis and aims to solve the problems that when an X-ray fluorescence spectrometer is used for measuring the weight of the zinc layer of a galvanized plate, the reliability of detection data is not high and manual secondary detection is needed when the detection range is large; the invention comprises the following steps: preparing standard samples with different contents, and accurately measuring the weight of a zinc layer of the standard samples by adopting a gravimetric method; respectively establishing a primary calibration curve measuring method and a secondary calibration curve measuring method on X-ray fluorescence instruments manufactured by manufacturers A and B by using the standard sample and the measuring result of the gravimetric method; respectively measuring the blind sample by using two X-ray fluorescence instruments, accurately measuring the blind sample by using a gravimetric method, and comparing results; the invention solves two defects in the primary calibration curve detection method, improves the reliability of the X fluorescence spectrometer on the detection data when the weight detection range of the zinc layer of the galvanized plate is larger, and reduces the workload of the detection personnel for secondary detection by a gravimetric method.
Description
Technical Field
The invention relates to the technical field of metallurgical material analysis, in particular to a method for measuring the weight of a zinc layer by an X-ray fluorescence method.
Background
At present, the weight of a zinc layer of a galvanized sheet is generally measured by an X-ray fluorescence method. When the weight of the zinc layer is measured by using an X-ray fluorescence spectrometer, a calibration curve needs to be established for describing the quantitative relation between the weight of the zinc layer and the X-ray fluorescence intensity measured by the instrument.
The calibration curve used in the determination of the weight of the zinc layer of the galvanized sheet by the X-ray fluorescence spectrometer is a primary calibration curve. The primary calibration curve method has two drawbacks. If a full-content calibration curve is established, the covered detection range is too large, the curve fitting degree is poor, and particularly, the difference between a high value and a low value and a standard value is large; secondly, if the calibration curves are established in a high calibration curve and a low calibration curve in a segmented manner, the calibration curves are troublesome, and the detection data of the intersection part of the segmented calibration curves are different, for example, the detection range of the current zinc layer weight is 30-160 g/square meter, the calibration curves are established once in the detection ranges of 30-90 g/square meter and 90-160 g/square meter respectively, when the zinc layer weight of the test sample is 80-100 g/square meter, the data obtained by the two calibration curves have certain difference and need to be subjected to chemical analysis for secondary inspection so as to determine the thickness of the test sample; in actual production, the thickness of the zinc layer of each grade of galvanized product is greatly different, the reliability of the result is not high, the inspection work is very complicated, and manual secondary detection is often needed. Therefore, a method for measuring the weight of the zinc layer by X-ray fluorescence is needed to solve the problem.
Disclosure of Invention
The invention aims to provide a method for measuring the weight of a zinc layer by an X-ray fluorescence method, which aims to solve the problems that when an X-ray fluorescence spectrometer is used for measuring the weight of the zinc layer of a galvanized plate, the reliability of detection data is not high, and manual secondary detection is needed when the detection range is large.
In order to achieve the purpose, the invention provides the following technical scheme: a method for measuring the weight of a zinc layer by an X-ray fluorescence method comprises the following specific steps:
s1, preparing standard samples with different contents according to the requirements of GB/T1839-2008 appendix A4.4, and accurately determining the weight of the zinc layer of the standard samples by adopting a weight method in GB/T1839-2008;
s2, respectively establishing a primary calibration curve measuring method and a secondary calibration curve measuring method on an X-ray fluorescence instrument manufactured by A manufacturer by using the measuring results of the standard sample and the gravimetric method;
s3, respectively establishing a primary calibration curve measuring method and a secondary calibration curve measuring method on an X-ray fluorescence instrument manufactured by a manufacturer B by using the measuring results of the standard sample and the gravimetric method;
and S4, measuring the blind sample by using the X-ray fluorescence instrument manufactured by the manufacturer A and the X-ray fluorescence instrument manufactured by the manufacturer B which establish the primary calibration curve measuring method and the secondary calibration curve measuring method respectively, accurately measuring the blind sample by using a gravimetric method, and comparing the results.
Preferably, the primary calibration curve is Ax + by + c is 0, and the secondary calibration curve is Ax2+Bxy+Cy2+ Dx + Ey + F ═ 0, where a, B, C, D, E, F are real numbers.
Preferably, the method further includes step S5, calculating correlation coefficients of the primary calibration curve and the secondary calibration curve of the X-ray fluorescence apparatus manufactured by manufacturer a and the X-ray fluorescence apparatus manufactured by manufacturer B, respectively.
Preferably, manufacturer A selects Marwinpanaceac, and manufacturer B selects Sammerfeier.
Preferably, the X-ray fluorescence instrument manufactured by manufacturer A has a correlation coefficient of 99.27% of a primary calibration curve and a correlation coefficient of 99.97% of a secondary calibration curve.
Preferably, the X-ray fluorometer manufactured by manufacturer B has a correlation coefficient of 99.17% for the primary calibration curve and 99.98% for the secondary calibration curve.
The invention provides another technical scheme that: a method for measuring the weight of a zinc layer by an X-ray fluorescence method comprises the following specific steps: preparing a standard sample, accurately measuring the weight of a zinc layer of the standard sample by adopting a gravimetric method, establishing a secondary calibration curve measuring method on an X-ray fluorescence instrument by using the standard sample and the measurement result of the gravimetric method, and measuring the sample to be measured by using the measuring method.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for measuring the weight of the zinc layer by using the X-ray fluorescence method, the accuracy and the effectiveness of the method are verified through different equipment, different methods, repeatability tests, reproducibility tests and calibration curve correlation coefficient comparison, the conclusion that the secondary calibration curve can improve the reliability of a detection result is finally obtained, two defects of a primary calibration curve method are overcome, and particularly the reliability of detection data when an X-ray fluorescence spectrometer is used for measuring the weight of the zinc layer of a galvanized plate in a large detection range is improved; in addition, the method is favorable for reducing the workload of detecting personnel for secondary detection by a gravimetric method, reducing the labor intensity, reducing the cost of human resources, relieving the problem of insufficient personnel, being powerful for optimizing inspection teams, and providing powerful support for improving the product quality of the hot galvanizing industry of companies.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
collecting internal control samples meeting daily production requirements according to the weight range of a zinc layer of a galvanized sheet corresponding to a production brand, covering a common range as far as possible, preparing standard samples with different contents according to the requirements of GB/T1839-2008 appendix A4.4, preferably preparing 5 standard samples, and accurately measuring the weight of the zinc layer of the standard samples by adopting a weight method in GB/T1839-2008;
respectively establishing a primary calibration curve measuring method and a secondary calibration curve measuring method on an X-ray fluorescence instrument of Malnpaneidae by using a standard sample and a measuring result of a gravimetric method (wherein the primary calibration curve is Ax + by + c is 0, and the secondary calibration curve is Ax)2+Bxy+Cy2+ Dx + Ey + F is 0, a, B, C, D, E, F are real numbers), schematically, the apparatus shows a quadratic calibration curve with x being 26.98515-0.25421y +0.00498y2When a is 0, C is 0.00498, D is-1, E is-0.25421, and F is 26.98515;
similarly, a primary calibration curve measuring method and a secondary calibration curve measuring method are respectively established on a Saimer Feishel X-ray fluorescence instrument by using the measurement results of the standard sample and the gravimetric method;
the two X-ray fluorescence instruments which establish the primary calibration curve measuring method and the secondary calibration curve measuring method are respectively used for measuring the blind sample, the blind sample is accurately measured by a gravimetric method, and the comparison results are shown in the following tables 1 and 2:
TABLE 1 Malverpa Nataceae X-ray fluorometer determination of blind samples
TABLE 2 Saimer Feishale X-ray fluorometer determination of blind samples
As can be seen from tables 1 and 2, the fitting between the secondary calibration curve and the weight of the zinc layer of the galvanized sheet was better and the reliability of the result was higher in any X-ray fluorometer.
Example 2:
the two X-ray fluorometers of example 1 were continuously used and the correlation coefficients of the primary calibration curve and the secondary calibration curve of the marvens parnacho X-ray fluorometer were calculated using the blind samples, and the sample values, the primary curve fit values and the secondary curve fit values are as follows:
| sample value | 34 | 40.4 | 51.1 | 65.5 | 71.2 | 80.2 | 90.7 |
| First order curve fitting value | 29 | 38 | 54 | 71 | 77 | 86 | 95 |
| Fitting value of quadratic curve | 34 | 40 | 52 | 65 | 72 | 80 | 91 |
| Sample value | 100.4 | 116.3 | 120.4 | 129.4 | 138 | 142.3 | 156 |
| First order curve fitting value | 104 | 116 | 120 | 127 | 131 | 137 | 146 |
| Fitting value of quadratic curve | 100 | 116 | 121 | 130 | 135 | 143 | 157 |
The correlation coefficient of the primary calibration curve and the correlation coefficient of the secondary calibration curve can be calculated to be 99.27% and 99.97%.
The correlation coefficients of the primary calibration curve and the secondary calibration curve of the Saimer Feishell X-ray fluorescence instrument are calculated by the same method, wherein the correlation coefficient of the primary calibration curve is 99.17%, and the correlation coefficient of the secondary calibration curve is 99.98%.
The correlation coefficients of the calibration curves of the two X-ray fluorescence instruments are both secondary calibration curves, and the secondary calibration curves are remarkably better.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (7)
1. A method for measuring the weight of a zinc layer by an X-ray fluorescence method is characterized by comprising the following specific steps:
s1, preparing standard samples with different contents according to the requirements of GB/T1839-2008 appendix A4.4, and accurately determining the weight of the zinc layer of the standard samples by adopting a weight method in GB/T1839-2008;
s2, respectively establishing a primary calibration curve measuring method and a secondary calibration curve measuring method on an X-ray fluorescence instrument manufactured by A manufacturer by using the measuring results of the standard sample and the gravimetric method;
s3, respectively establishing a primary calibration curve measuring method and a secondary calibration curve measuring method on an X-ray fluorescence instrument manufactured by a manufacturer B by using the measuring results of the standard sample and the gravimetric method;
and S4, measuring the blind sample by using the X-ray fluorescence instrument manufactured by the manufacturer A and the X-ray fluorescence instrument manufactured by the manufacturer B which establish the primary calibration curve measuring method and the secondary calibration curve measuring method respectively, accurately measuring the blind sample by using a gravimetric method, and comparing the results.
2. The method for measuring the weight of a zinc layer by an X-ray fluorescence method according to claim 1, wherein the method comprises the following steps: the primary calibration curve is Ax + by + c is 0, and the secondary calibration curve is Ax2+Bxy+Cy2+ Dx + Ey + F ═ 0, where a, B, C, D, E, F are real numbers.
3. The method for measuring the weight of a zinc layer by an X-ray fluorescence method according to claim 1, wherein the method comprises the following steps: the method further includes step S5, calculating correlation coefficients of the first calibration curve and the second calibration curve of the X-ray fluorometer manufactured by manufacturer a and the X-ray fluorometer manufactured by manufacturer B, respectively.
4. The method for measuring the weight of a zinc layer by an X-ray fluorescence method according to claim 3, wherein the method comprises the following steps: the manufacturer A selects Marvinparnaceae, and the manufacturer B selects Sammer Feishel.
5. The method of claim 4, wherein the weight of the zinc layer is determined by X-ray fluorescence method, and the method comprises the following steps: the X-ray fluorescence instrument manufactured by the manufacturer A has a correlation coefficient of a primary calibration curve of 99.27 percent and a correlation coefficient of a secondary calibration curve of 99.97 percent.
6. The method of claim 4, wherein the weight of the zinc layer is determined by X-ray fluorescence method, and the method comprises the following steps: the X-ray fluorescence instrument manufactured by the manufacturer B has a correlation coefficient of a primary calibration curve of 99.17 percent and a correlation coefficient of a secondary calibration curve of 99.98 percent.
7. A method for measuring the weight of a zinc layer by an X-ray fluorescence method is characterized by comprising the following specific steps: preparing a standard sample, accurately measuring the weight of a zinc layer of the standard sample by adopting a gravimetric method, establishing a secondary calibration curve measuring method on an X-ray fluorescence instrument by using the standard sample and the measurement result of the gravimetric method, and measuring the sample to be measured by using the measuring method.
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Citations (6)
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| JPS6161003A (en) * | 1984-09-03 | 1986-03-28 | Seiko Instr & Electronics Ltd | Method and instrument for measuring thickness of plating layer by x rays |
| JPH05203593A (en) * | 1992-01-28 | 1993-08-10 | Nisshin Steel Co Ltd | Method and device for measuring plating adhesion quantity |
| CN104569019A (en) * | 2015-01-20 | 2015-04-29 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | Method for measuring content of metal elements in copper anode mud |
| CN105510370A (en) * | 2016-02-22 | 2016-04-20 | 芜湖东旭光电装备技术有限公司 | Method for measuring content of main ingredients in stannic oxide electrode block |
| CN108918566A (en) * | 2018-08-06 | 2018-11-30 | 酒泉钢铁(集团)有限责任公司 | A kind of method of inspection for plating zinc-aluminum-magnesium plate coating |
| CN110596170A (en) * | 2019-09-17 | 2019-12-20 | 陕西延长中煤榆林能源化工有限公司 | Method for measuring thermoplastic ash content by wavelength dispersion X-ray fluorescence spectrometry |
-
2021
- 2021-11-17 CN CN202111359403.1A patent/CN114047213A/en active Pending
Patent Citations (6)
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|---|---|---|---|---|
| JPS6161003A (en) * | 1984-09-03 | 1986-03-28 | Seiko Instr & Electronics Ltd | Method and instrument for measuring thickness of plating layer by x rays |
| JPH05203593A (en) * | 1992-01-28 | 1993-08-10 | Nisshin Steel Co Ltd | Method and device for measuring plating adhesion quantity |
| CN104569019A (en) * | 2015-01-20 | 2015-04-29 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | Method for measuring content of metal elements in copper anode mud |
| CN105510370A (en) * | 2016-02-22 | 2016-04-20 | 芜湖东旭光电装备技术有限公司 | Method for measuring content of main ingredients in stannic oxide electrode block |
| CN108918566A (en) * | 2018-08-06 | 2018-11-30 | 酒泉钢铁(集团)有限责任公司 | A kind of method of inspection for plating zinc-aluminum-magnesium plate coating |
| CN110596170A (en) * | 2019-09-17 | 2019-12-20 | 陕西延长中煤榆林能源化工有限公司 | Method for measuring thermoplastic ash content by wavelength dispersion X-ray fluorescence spectrometry |
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